반응 #56947

ord-79a94e99805e44c78a5760e8bf40445b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 18 h
  2. 2
    농축concentrated under reduced pressure
  3. 3
    기타The solid residue was triturated with cold water
  4. 4
    추출extracted with DCM
  5. 5
    세척The extract was washed with water, aqueous brine solution
  6. 6
    건조dried over MgSO4
  7. 7
    농축concentrated in vacuo

실험 절차

Thionyl chloride (10 mL, 0.137 mol) was added dropwise to a stirred suspension of the 1-bromophenyl-1H-benzimidazole-5-carboxylic acid (20 g, 0.063 mol) in MeOH (200 mL) at 0-5° C. The reaction was stirred at reflux for 18 h and then concentrated under reduced pressure. The solid residue was triturated with cold water, basified with aqueous ammonium hydroxide solution and extracted with DCM. The extract was washed with water, aqueous brine solution, dried over MgSO4 and concentrated in vacuo to give the corresponding 1-bromophenyl-1H-benzimidazole-5-carboxylic acid methyl ester: e.g. 1-(4-bromophenyl)-1H-benzimidazole carboxylic acid methyl ester.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07419995B2uspto-grants-2008_09